反応 #824118

反応方程式

HCl

diethyl 2-acetylamino-2-(4-amino-3-chloro-5-trifluoromethyl-benzyl)-malonate

→

2-amino-3-(4-amino-3-chloro-5-trifluoromethyl-phenyl)-propionic acid-hydrochloride

溶媒

AcOH

water

反応条件

後処理

1. 1
   その他The precipitate formed
2. 2
   ろ過was filtered off
3. 3
   その他The filtrate was evaporated down i
4. 4
   その他The precipitate formed
5. 5
   ろ過was filtered off
6. 6
   洗浄washed with EtOH
7. 7
   その他dried i
8. 8
   その他The crude product was used in the next reaction step without any further purification

実験手順

50 mL conc. HCl were added to a solution of 40.0 g (94.16 mmol) of diethyl 2-acetylamino-2-(4-amino-3-chloro-5-trifluoromethyl-benzyl)-malonate in 110 mL AcOH and 150 mL of water and the reaction mixture was heated to 140° C. for 4 h. The precipitate formed was filtered off and discarded. The filtrate was evaporated down i. vac., combined with 100 mL of EtOH and stirred for 15 min at RT. The precipitate formed was filtered off, washed with EtOH and dried i. vac. The crude product was used in the next reaction step without any further purification.

出典